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Method for preparation of sugammadex sodium with polymer-loaded trivalent phosphine compound

A technology of sugammadex sodium and phosphine compounds, which is applied in the pharmaceutical field, can solve the problems of synthesis and purification of sugammadex sodium, which have not been seen, and achieve the effects of high environmental protection significance and economic value, easy purification, and improved economy.

Active Publication Date: 2019-08-23
郭辉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0019] At present, there is no corresponding literature on the application of polymer-loaded trivalent phosphine compounds to the synthesis and purification of sugammadex sodium

Method used

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  • Method for preparation of sugammadex sodium with polymer-loaded trivalent phosphine compound
  • Method for preparation of sugammadex sodium with polymer-loaded trivalent phosphine compound
  • Method for preparation of sugammadex sodium with polymer-loaded trivalent phosphine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1. Synthesis of 6-deoxy-6-periodo-γ-cyclodextrin

[0057] Under stirring, add cross-linked polystyrene supported triphenylphosphine resin (60.2g), anhydrous DMF (160ml) and iodine (30.5g, 15.6 equivalents) into the flask, and the system exotherms. Dried γ-cyclodextrin (10 g, 7.7 mmol) was added, and the temperature was raised to 70° C. to react for 24 hours. After the reaction is over, cool the system, remove the crosslinked polystyrene-loaded triphenylphosphine resin by suction filtration, add methanol solution of sodium methylate (3.1g sodium is dissolved in 50ml methanol) in the filtrate, stir for 30 minutes, and add it to 800ml methanol medium, suction filtered, and the filter cake was dried. Add 500ml of water to the residue, filter with suction, wash the filter cake with water (3*100ml), and then wash with acetone (3*100ml), and dry it in vacuum at 70°C to obtain yellow 6-perdeoxy-6-periodo- Gamma-cyclodextrin solid (16.2 g). The recovered cross-linked polystyr...

Embodiment 2

[0063] 1. Synthesis of 6-deoxy-6-perbromo-γ-cyclodextrin

[0064] Under stirring, add cross-linked polystyrene supported triphenylphosphine resin (60.2g), anhydrous DMF (160ml) into the flask, and add bromine (19.2g, 15.6 equivalents) dropwise, and the system exotherms. Dried γ-cyclodextrin (10 g, 7.7 mmol) was added, and the temperature was raised to 70° C. to react for 24 hours. After the reaction is over, cool the system, remove the crosslinked polystyrene-loaded triphenylphosphine resin by suction filtration, add methanol solution of sodium methylate (3.1g sodium is dissolved in 50ml methanol) in the filtrate, stir for 30 minutes, and add it to 800ml methanol medium, suction filtered, and the filter cake was dried. Add 500ml of water to the residue, filter with suction, wash the filter cake with water (3*100ml), and then wash with acetone (3*100ml), and dry it in vacuum at 70°C to obtain yellow 6-perdeoxy-6-perbromo- Gamma-cyclodextrin solid (13.2 g). The recovered cros...

Embodiment 3

[0070] 1. Synthesis of 6-deoxy-6-perchloro-γ-cyclodextrin

[0071] Under stirring, add cross-linked polystyrene supported triphenylphosphine resin (60.2g), anhydrous DMF (160ml) and carbon tetrachloride (18.5g, 15.6 equivalents) into the flask, and the system exotherms. Dried γ-cyclodextrin (10 g, 7.7 mmol) was added, and the temperature was raised to 60° C. to react for 40 hours. After the reaction is over, cool the system, remove the crosslinked polystyrene-loaded triphenylphosphine resin by suction filtration, add methanol solution of sodium methylate (3.1g sodium is dissolved in 50ml methanol) in the filtrate, stir for 30 minutes, and add it to 800ml methanol medium, suction filtered, and the filter cake was dried. Add 500ml of water to the residue, filter with suction, wash the filter cake with water (3*100ml), and then wash with acetone (3*100ml), and dry it in vacuum at 70°C to obtain yellow 6-perdeoxy-6-perchloro- Gamma-cyclodextrin solid (16.2 g). The recovered cro...

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Abstract

The invention discloses a method for synthesis and purification of sugammadex sodium with a polymer-loaded trivalent phosphine compound. The polymer-loaded trivalent phosphine compound is employed tosubstitute triphenylphosphine to synthesize a sugammadex sodium crude product, and the polymer-loaded trivalent phosphine compound is applied to the purification process of the sugammadex sodium crudeproduct, the obtained sugammadex sodium finished product has purity up to 100.0% (including monohydroxy sugammadex sodium), and the single impurity is less than 0. 1%. The method provided by the invention meets the requirements of green chemistry, and has high environmental protection significance and economic value.

Description

technical field [0001] The invention belongs to the technical field of pharmacy and relates to a preparation method of sugammadex sodium, in particular to a method for synthesizing and purifying sugammadex sodium by using a polymer loaded trivalent phosphine compound. Background technique [0002] The chemical name of sugammadex sodium is 6A, 6B, 6C, 6D, 6E, 7F, 6G, 6H-octa-S-(2-carboxyethyl)-6A, 6B, 6C, 6D, 6E, 7F, 6G, 6H-octathio-γ-cyclodextrin, octasodium salt, its molecule consists of a lipophilic core and a hydrophilic outer end, the structure of the compound is as follows: [0003] [0004] Sugammadex sodium is a new type of muscle relaxant reversal agent developed by Organon in the Netherlands. It is clinically used to reverse the neuromuscular blockade of rocuronium or vecuronium. It has a good curative effect and has excellent security. Since the European Union approved its listing in July 2008, it has been listed in Japan, South Korea, the United States and ot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16
CPCC08B37/0003C08B37/0012
Inventor 郭辉
Owner 郭辉
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